6 Materialchemie
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The presentation summarizes our recent results on the coupled electrochemical methods for high resolution corrosion studies. The combination of Scanning Electrochemical Microscopy (SECM) and multielectrode (MMA) based real-time corrosion monitoring was presented as a new method for achieving high time resolution in local electrochemical analysis. Correlative imaging by means of Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM) was demonstrated as a tool for the investigation of local corrosion processes initiated by the intermetallic particles (IMPs) on AA2024-T3 aluminium alloy.
The performance of functional coatings and adhesively joined hybrid components relies strongly on the stability of the polymer-metal interface. With the increasing utilization of multi-material structures in the automotive and aerospace industry, it is of great scientific and technical interest to understand the processes leading to interface degradation and to develop novel strategies to increase corrosion and delamination resistance.
The aim of this project is to develop thin epoxy-based films and their carbon nanofiller loaded composites on aluminium alloy AA2024-T3 as a model system and to investigate their interfacial stability under corrosive and coupled corrosive-mechanical load. Spin coating was used for the layer-by-layer deposition of poly[(o-cresyl glycidyl ether)-co-formaldehyde] and poly-(ethylenimine) bi-layers. Atomic force microscopy (AFM) results indicate a very homogeneous and dense film with low surface roughness. Carbon nanofillers were introduced either by mixing into the coating components or in between individual layers to control the separation between the carbon nanofillers and alloy surface. The film chemistry and barrier properties were characterized by means of spectroscopic and electrochemical methods, respectively. The degradation and delamination behavior of the epoxy-based films was characterized by means of in situ AFM corrosion experiments. The quantitative imaging (QI) mode allowed the observation of hydrogen-generation induced blister formation during exposure to corrosive electrolyte and how the local corrosion processes evolved with exposure time. Complementary energy dispersive X-ray spectroscopy (EDX) analysis was performed to correlate the corrosion behavior with the different intermetallic particle chemistries and distributions. The presentation will summarize our results on the effect of interface chemistry and carbon nanofiller – alloy separation on the initiation of local corrosion processes on thin film covered AA2024-T3 aluminium alloys.
In service, most materials are operated under simultaneous corrosive and mechanical load and there are very few methods capable for testing material degradation under these conditions, especially when it comes to high resolution analysis. For this purpose, in this work, a tensile module capable of uniaxial stretching and compression with up to 5 kN force was integrated into an AFM stage. The elimination of the need for sample unmounting and remounting and the resulting possibility of keeping the sample under constant mechanical load during AFM measurements not only enables a precise positioning of the area of interest but also allows for the analysis of processes in the elastic deformation regime.
This methodology was demonstrated for two case studies. Scanning Kelvin Probe Force Microscopy (SKPFM) was used as the main tool to characterize the deformation behavior. Moreover, a flexible electrochemical measurement cell was used to enable electrochemical analysis by means of electrochemical impedance spectroscopy (EIS) and Linear Sweep Voltammetry (LSV) during AFM measurements at different levels of strain. The in situ AFM results are complemented by microstructure analysis by means of electron backscatter diffraction (EBSD).
In the first case study, the deformation induced delamination of a thin organic coating on AA2024 T3 aluminium alloy was investigated as a function of alloy surface treatment. The formation of cracks in the insulating passive film enabled an early detection of deformation processes by means of SKPFM. The second case study focused on the comparison of corrosion and deformation behavior of conventional and additively manufactured 316 stainless steels. In comparison to the conventional 316 stainless steel, the effect of processing was clearly detectable on the additively manufactured material as zones of inhomogeneous potential, which also affected the initiation of local corrosion processes. The contribution will provide detailed information on the new AFM setup and summarize our results from both case studies.
Selection and study of alkoxysilanes as loading in submicrocapsules for self-lubricating coatings
(2019)
The possibility and conditions for the formation of nano- or submicrocapsules loaded with hydrophobic active ingredients (alkoxysilanes) into the matrix of coatings with self-lubricating effect are considered. The optimal composition of the alkoxysilane submicrocapsules, and their physicochemical properties were determined. The longer the radical chain length is, the lower is the rate of hydrolysis, and, accordingly, the more stable is the formed emulsion. The methods of laser correlation spectroscopy in measuring the size and zeta potentials of the submicrocapsules with different loads of the active agent allowed to determine the optimal ratios of the active ingredients. The optimal concentration of the active agent is between 4 and 9%. Based on contact angle studies, octadecyltrimethoxysilane was selected as optimum compound. The introduction of 4 wt% of octadecyltrimethoxysilane reduces the friction coefficient of coatings by 20–30% under vibrating motion and by 15–20% under continuous motion. The data obtained can also be useful for the encapsulation of other hydrophobic active agents and for various other purposes, for example, for the introduction of biocidal agents.
Microbiologically induced corrosion due to bacterial biofilms causes several problems in industrial systems, technical applications and in medicine. Prior to the formation of a biofilm on a substrate, planktonic cells attach on the surface. Hence, the properties of the surface play a key role in biofilm formation and are of great importance for the development of strategies to prevent bacterial attachment and biofilm formation.
This project aims at clarifying to which extent surface micro-/nanostructuring and chemical functionalization affects bacterial attachment and whether a synergistic combination of the two can be used to control bacterial adhesion. To answer these questions, model surfaces with regular patterns of 5-10 micrometers in size have been prepared, which provide distinct zones differing in terms of their chemistry or nano-roughness. This was achieved by micro contact printing of self-assembled monolayers with different functional groups and deposition of patterned ZnO nanorod arrays for studying the effect of surface chemistry and morphology, respectively. Typical contrasts studied were combinations of positively/negatively charged, hydrophobic/hydrophilic or flat/rough.
The attachment behavior of bacteria on tailored surfaces were studied in a flow chamber as a function of time. The strain Pseudomonas fluorescens SBW25 was chosen as a model organism. DNA-intercalating dyes such as Syto9 have a high affinity to adsorb on ZnO nanorods. To overcome this limitation a genetic modification was performed by introducing a gene which expresses a green fluorescent protein in P. fluorescens SBW25 enabling the quantitative evaluation of the flow chamber studies by means of fluorescence microscopy. Further analysis of the attachment behavior was performed by means of scanning electron microscopy.
The presentation will summarize the results of our systematic study on the role of individual parameters on bacterial attachment and highlight synergistic combinations, showing an inhibition or enhancing effect. As the investigations with model substrates enable a precise control of the surface parameters, this approach can be applied to different microorganisms and material systems to achieve a correlative description of bacterial adhesion on solid surfaces.
In this study, femtosecond laser-induced sub-micrometer structures are generated to modify polyethylene (PE) surface topographies. These surfaces were subjected to bacterial colonization studies with Escherichia coli and Staphylococcus aureus as test strains. The results reveal that the nanostructures do not influence S. aureus coverage, while the adhesion of E. coli is reduced.
The formation of gratings on the surface of a silicon wafer by nanosecond laser irradiation through a phase mask using an ArF laser emitting at 193 nm is studied. The phase mask along with some focusing optics is capable to generate via interference a periodic intensity distribution, which can be used for surface patterning. The surface patterning strongly depends on the laser energy density and on the number of pulses, as revealed by atomic force microscopy (AFM). The results show that irradiation even with a single laser pulse produces periodic depth modulations on the surface. The spatial surface modulation is in the micrometer (1.7 µm) range while the depth modulation is in the nanometer regime (1–20 nm). With an increasing number of pulses (1–100), the depth modulation amplitude increases smoothly. Increasing the number of pulses further results in the progressive destruction of the grating, vanishing completely after ~5000 pulses. This evolution is also monitored in situ by measuring the intensity of the first order-diffracted probe beam and the behavior is in accordance with what is observed by AFM. Finally, we qualitatively explain the results invoking thermally induced effects in the melted Si: these physical processes involved are probably thermocapillary and/or Marangoni effects inducing material displacement as the surface melts.
In this paper, the influence of the bulk temperature (BT) of Polycarbonate (PC) on the occurrence and growth of Laser-induced Periodic Surface Structures (LIPSS) is studied. Ultrashort UV laser pulses with various laser peak fluence levels F_0 and various numbers of overscans (N_OS) were applied on the surface of pre-heated Polycarbonate at different bulk temperatures. Increased BT leads to a stronger absorption of laser energy by the Polycarbonate. For N_OS < 1000 High Spatial Frequency LIPSS (HSFL), Low Spatial Frequency LIPSS perpendicular (LSFL-I) and parallel (LSFL-II) to the laser polarization were only observed on the rim of the ablated tracks on the surface but not in the center of the tracks. For N_OS ≥ 1000 , it was found that when pre-heating the polymer to a BT close its glass transition temperature (T_g), the laser fluence to achieve similar LIPSS as when processed at room temperature decreases by a factor of two. LSFL types I and II were obtained on PC at a BT close to T_g and their periods and amplitudes were similar to typical values found in the literature. To the best of the author’s knowledge, it is the first time both LSFL types developed simultaneously and consistently on the same sample under equal laser processing parameters. The evolution of LIPSS from HSFL, over LSFL-II to LSFL I, is described, depending on laser peak fluence levels, number of pulses processing the spot and bulk temperature.